麸炒白术配方颗粒特征图谱及白术内酯Ⅲ含量测定研究

Study on HPLC Specific Chromatogram of Bran-processed Atractylodes Formula Granule and Determination of Atractylenolide Ⅲ

目的建立麸炒白术饮片和麸炒白术配方颗粒中白术内酯Ⅲ的含量测定方法,并同时建立麸炒白术配方颗粒的HPLC特征图谱。方法采用色谱柱为Welch Xtimate C18柱(250 mm×4.6 mm,5μm);流动相为乙腈-水溶液,梯度洗脱;体积流量1.0 m L·min^(-1);柱温30℃;检测波长224 nm;进样量10μL。结果建立了麸炒白术饮片及颗粒中白术内酯Ⅲ的含量测定方法,白术内酯Ⅲ在0.031 3~0.782 4μg内与色谱峰面积呈良好的线性关系;麸炒白术饮片和麸炒白术配方颗粒平均加样回收率分别102.0%(RSD=1.88%),101.0%(RSD=1.02%);建立了麸炒白术配方颗粒的HPLC特征图谱,确立了8个特征峰。结论该方法准确、可靠,为麸炒白术配方颗粒的工艺研究及质量控制提供了参考依据。

OBJECTIVE To establish an HPLC method for the determination of atractylenolide Ⅲin bran-processed atractylodes and bran-processed Atractylodes Formula granule, and to establish the specific chromatogram of bran-processed Atractylodes Formula granule. METHODS The chromatographic separation was performed on a Welch Xtimate C_（18） column（250 mm×4.6 mm, 5 μm）. The mobile phase was a mixture of acetonitrile-water in gradient elution at a flow rate of 1.0 m L·min^（-1）. The detection wavelength was 224 nm and the column temperature was set at 30 ℃. RESULTS The linear range of atractylenolide in branⅢ-processed atractylodes and bran-processed Atractylodes Formula granule was 0.031 3-0.782 4 μg, with average recovery of 102.0%（RSD=1.88%） and 101.0%（1.02%）. The HPLC specific chromatogram of bran-processed Atractylodes Formula granule showed 8 characteristic peaks. CONCLUSION The method is reliable and accurate, and can provide a reference for the technical study and quality control of bran-processed Atractylodes Formula granule.